大豆中6种磺酰脲类除草剂残留量的高效液相色谱-质谱法测定  

Determination of Six Sulfonylurea Herbicide Residues in Soybeans by HPLC-MS

作　　者：祁彦[1] 张新忠[2] 杨强[1] 雍炜[1] 

机构地区：[1]中国检验检疫科学研究院,北京100025 [2]中国农业大学理学院,北京100094

出　　处：《分析测试学报》2005年第4期54-57,60,共5页Journal of Instrumental Analysis

基　　金：国家科技基础条件平台重点项目资助(2003DIA6N003)

摘　　要：建立了LC-MS选择离子监测(SIM)同时检测大豆中6种磺酰脲类除草剂残留量的方法.样品经乙腈提取,正己烷液-液分配,Florisil柱净化,然后采用HPLC-ESI(+)-MS测定.6种磺酰脲类除草剂在25～1 000μg/L范围内线性良好,相关系数为0.999 6～0.999 7.在0.02～1.0 mg/kg范围内,平均加标回收率在72%～99%之间,相对标准偏差为0.9%～7.7%.方法的检出限低于10μg/kg.A high performance liquid chromatography/electrospray ionization mass spectrometry method at the selective ion monitoring mode has been developed for the simultaneous determination of six sulfonylurea herbi-cide residues in soybeans.Sulfonylurea herbicides were extracted with acetonitrile,followed by hexane parti-tioning.After the extract was cleaned up with florisil column,sulfonylurea herbicides were analyzed by HPLC-ESI(+)-MS and quantified by external calibration method.The linear range was from0.025to 1.0μg/mL,and the correlation coefficients were0.9996-0.9997.The average recoveries of six sulfony-lurea herbicides in spiked soybeans ranged from72%to99%,and the relative standard deviations were be-tween0.9%and7.7%.The detection limit of this method was10μg/kg.

关 键 词：除草剂 磺酰脲类 大豆 高效液相色谱-质谱法 

分 类 号：O657.63[理学—分析化学] O657.72[理学—化学]